COLORIMETRIC SOLUTIONS (CS)
(For the Preparation of Matching Fluids, see Color and Achromicity 631.)
These solutions are used in the preparation of the colorimetric standards for certain drugs, and for the carbonization tests with sulfuric acid that are specified in several monographs. Store the solutions in suitably resistant, tight containers.
Comparison of colors as directed in the Pharmacopeial tests preferably is made in matched color-comparison tubes or in a suitable colorimeter under conditions that ensure that the colorimetric reference solution and that of the specimen under test are treated alike in all respects. The comparison of colors is best made in layers of equal depth, and viewed transversely against a white background (see also Visual Comparison under Spectrophotometry and Light-Scattering 851). It is particularly important that the solutions be compared at the same temperature, preferably 25.
Cobaltous Chloride CS —Dissolve about 65 g of cobaltous chloride (CoCl2·6H2O) in enough of a mixture of 25 mL of hydrochloric acid and 975 mL of water to make 1000 mL. Pipet 5 mL of this solution into a 250-mL iodine flask, add 5 mL of hydrogen peroxide TS and 15 mL of sodium hydroxide solution (1 in 5), boil for 10 minutes, cool, and add 2 g of potassium iodide and 20 mL of dilute sulfuric acid (1 in 4). When the precipitate has dissolved, titrate the liberated iodine with 0.1 N sodium thiosulfate VS, adding 3 mL of starch TS as the indicator. Perform a blank determination with the same quantities of the same reagents, and make any necessary correction. Each mL of 0.1 N sodium thiosulfate is equivalent to 23.79 mg of CoCl2·6H2O. Adjust the final volume of the solution by the addition of enough of the mixture of hydrochloric acid and water so that each mL contains 59.5 mg of CoCl2.6H2O.
Cupric Sulfate CS —Dissolve about 65 g of cupric sulfate (CuSO4·5H2O) in enough of a mixture of 25 mL of hydrochloric acid and 975 mL of water to make 1000 mL. Pipet 10 mL of this solution into a 250-mL iodine flask, add 40 mL of water, 4 mL of acetic acid, 3 g of potassium iodide, and 5 mL of hydrochloric acid, and titrate the liberated iodine with 0.1 N sodium thiosulfate VS, adding 3 mL of starch TS as the indicator. Perform a blank determination with the same quantities of the same reagents, and make any necessary correction. Each mL of 0.1 N sodium thiosulfate is equivalent to 24.97 mg of CuSO4·5H2O. Adjust the final volume of the solution by the addition of enough of the mixture of hydrochloric acid and water so that each mL contains 62.4 mg of CuSO4.5H2O.
Ferric Chloride CS —Dissolve about 55 g of ferric chloride (FeCl3.6H2O) in enough of a mixture of 25 mL of hydrochloric acid and 975 mL of water to make 1000 mL. Pipet 10 mL of this solution into a 250-mL iodine flask, add 15 mL of water, 3 g of potassium iodide, and 5 mL of hydrochloric acid, and allow the mixture to stand for 15 minutes. Dilute with 100 mL of water, and titrate the liberated iodine with 0.1 N sodium thiosulfate VS, adding 3 mL of starch TS as the indicator. Perform a blank determination with the same quantities of the same reagents, and make any necessary correction. Each mL of 0.1 N sodium thiosulfate is equivalent to 27.03 mg of FeCl3.6H2O. Adjust the final volume of the solution by the addition of enough of the mixture of hydrochloric acid and water so that each mL contains 45.0 mg of FeCl3.6H2O.